CN104174303B - Enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane and preparation method thereof - Google Patents
Enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane and preparation method thereof Download PDFInfo
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- CN104174303B CN104174303B CN201410423395.6A CN201410423395A CN104174303B CN 104174303 B CN104174303 B CN 104174303B CN 201410423395 A CN201410423395 A CN 201410423395A CN 104174303 B CN104174303 B CN 104174303B
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Abstract
The invention discloses a kind of enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane and preparation method thereof；It is filled with enhancement fiber in the membranous wall of described enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane；The preparation method of described enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane comprises the following steps: 1) Kynoar, solvent and additive mix and blend are configured to preparation liquid；2) deaeration after preparation liquid being filtered；3) preparation liquid after deaeration is extruded by spinneret, continuous print enhancement fiber is introduced in the preparation liquid of spinneret simultaneously and extrude together with preparation liquid；4) as-spun fibre of extrusion is immersed in coagulating bath it is frozen into hollow-fibre membrane；5) put into hollow-fibre membrane glycerin solution soaks and protect hole, be then placed in water soaking.The present invention makes the intensity of polyvinylidene fluoride hollow fiber ultrafiltration membrane be strengthened, and also will not destroy the microcellular structure of film or make the microcellular structure of film change simultaneously, improve service life and practicality.
Description
Technical field
The invention belongs to technical field of membrane separation, be specifically related to a kind of enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane and preparation method thereof.
Background technology
Membrane separation technique is the new separation technology of a kind of green high-efficient, and ultrafiltration has bright prospects in Water warfare, chemical separating and bio-separation field.Hollow fiber ultrafiltration membrane is a kind of widely used filter medium, and the material that it can be removed includes biomolecule, high molecular polymer, colloidal substance, can realize reclaiming, concentrates, the technical process such as extraction.Density is big, device volume is little, energy consumption is low, use the advantages such as easy to operate in hollow fiber ultrafiltration membrane filling, is widely used in the industry fields such as biology, pharmacy, food, chemical industry, metallurgy and waste water control.
Kynoar (PVDF) hollow fiber ultrafiltration membrane receives much concern with its good corrosion resistance, solvent resistance and temperature tolerance and the feature such as easily prepared, and it is widely used in waste water control.But, now widely used polyvinylidene fluoride hollow fiber ultrafiltration membrane has obvious defect, the most intensity of this milipore filter is low, poor rigidity, under low pressure it is susceptible to deformation, affect filtering accuracy and flux, serious it also occur that holes and fracture of wire, it is impossible to meet the immersion type membrane component use requirement of strength to hollow-fibre membrane.Therefore research and develop a kind of new enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane, have a very important role.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane and preparation method thereof, the intensity of polyvinylidene fluoride hollow fiber ultrafiltration membrane is strengthened, and improves its service life and practicality.
For reaching above-mentioned purpose, the present invention provides following technical scheme:
The invention discloses a kind of enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane, in the membranous wall of described polyvinylidene fluoride hollow fiber ultrafiltration membrane, be filled with enhancement fiber.
Further, described enhancement fiber is organic fiber or inorfil.
Further, described organic fiber is aromatic polyamide fibre, superhigh molecular weight polyethylene fibers or Poly-p-phenylene benzobisthiazole.
Further, described inorfil is glass fibre, carbon fiber, boron fibre, ceramic fibre or metallic fiber.
Further, a diameter of 0.1 ~ 10 μm of described enhancement fiber.
Further, described enhancement fiber cincture distribution in the membranous wall of polyvinylidene fluoride hollow fiber ultrafiltration membrane.
The invention also discloses the preparation method of described enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane, comprise the following steps:
1) Kynoar, solvent and additive mix and blend are configured to preparation liquid；
2) deaeration after preparation liquid filtration step 1) obtained；
3) by step 2) preparation liquid after deaeration extruded by spinneret, and continuous print enhancement fiber is introduced in the preparation liquid of spinneret and extrudes together with preparation liquid simultaneously；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane.
Further, in described step 1), the mass ratio of Kynoar, solvent and additive is 10 ~ 30:70 ~ 90:1 ~ 10, and the stirring preparation temperature of preparation liquid is 50 ~ 85 DEG C.
Further, in described step 1), solvent one in dimethylformamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, triethyl phosphate, trimethyl phosphate, hexamethyl ammonium phosphate, tetramethylurea, oxolane and acetone, additive one in polyvinylpyrrolidone, polyethylene glycol, lithium chloride, lithium perchlorate, glycerine, ethylene glycol, methyl alcohol, ethanol, water, formic acid and ethyl acetate.
Further, in described step 3), enhancement fiber constantly rotates when introducing in the preparation liquid of spinneret, makes enhancement fiber around distribution in the preparation liquid of spinneret.
The beneficial effects of the present invention is:
The present invention is by filling enhancement fiber in the membranous wall of polyvinylidene fluoride hollow fiber ultrafiltration membrane, the intensity making polyvinylidene fluoride hollow fiber ultrafiltration membrane is strengthened, also will not destroy the microcellular structure of film or make the microcellular structure of film change simultaneously, thus improve the number of backwashes of polyvinylidene fluoride hollow fiber ultrafiltration membrane, improve service life and practicality.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and beneficial effect clearer, the preferred embodiments of the present invention will be described in detail below.
Embodiment
1
1) adding Kynoar, 1-METHYLPYRROLIDONE and polyethylene glycol (PEG-6000) in a kettle., mass ratio is 20:77:3, and at 55 DEG C, stirring makes it dissolve, and stirs 24h, forms uniform preparation liquid；
2) preparation liquid step 1) obtained filters through 200 mesh steel meshes, then by preparation liquid at room temperature vacuumizing and defoaming；
3) by step 2) preparation liquid after deaeration is at the N of 0.3MPa2Extruded by spinneret under pressure, a glass fibre of a diameter of 0.1 μm of rolling is introduced in the preparation liquid of spinneret simultaneously and extrude together with preparation liquid；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane.
The enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane that embodiment 1 obtains, is filled with glass fibre in its membranous wall；The porosity recording this enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane is 83%, and under 0.2Mpa permeable membrane pressure reduction, pure water flux is 193.43L m-2·h-1, average pore size is in 0.036 μm, and hot strength is 6.38N, and elongation at break is 6.3%.
Embodiment
2
1) adding Kynoar, 1-METHYLPYRROLIDONE and polyethylene glycol (PEG-6000) in a kettle., mass ratio is 20:77:3, and at 55 DEG C, stirring makes it dissolve, and stirs 24h, forms uniform preparation liquid；
2) preparation liquid step 1) obtained filters through 200 mesh steel meshes, then by preparation liquid at room temperature vacuumizing and defoaming；
3) by step 2) preparation liquid after deaeration is at the N of 0.3MPa2Being extruded by spinneret under pressure, introduced by a glass fibre of a diameter of 0.1 μm of rolling in the preparation liquid of spinneret simultaneously, glass fibre constantly rotates under the effect of drawing head, around distribution and extrudes together with preparation liquid in the preparation liquid of spinneret；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane.
The enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane that embodiment 2 obtains, is filled with glass fibre, and glass fibre is around distribution, forms the reinforcement of a cincture in its membranous wall；The porosity recording this enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane is 80%, and under 0.2Mpa permeable membrane pressure reduction, pure water flux is 186.16L m-2·h-1, average pore size is in 0.031 μm, and hot strength is 7.42N, and elongation at break is 5.4%.
Embodiment
3
1) adding Kynoar, 1-METHYLPYRROLIDONE and polyethylene glycol (PEG-6000) in a kettle., mass ratio is 20:77:3, and at 55 DEG C, stirring makes it dissolve, and stirs 24h, forms uniform preparation liquid；
2) preparation liquid step 1) obtained filters through 200 mesh steel meshes, then by preparation liquid at room temperature vacuumizing and defoaming；
3) by step 2) preparation liquid after deaeration is at the N of 0.3MPa2Extruded by spinneret under pressure, three glass fibres of a diameter of 0.1 μm of rolling are introduced in the preparation liquid of spinneret simultaneously and extrude together with preparation liquid；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane.
The enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane that embodiment 3 obtains, is filled with glass fibre in its membranous wall；The porosity recording this enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane is 79%, and under 0.2Mpa permeable membrane pressure reduction, pure water flux is 171.13L m-2·h-1, average pore size is in 0.029 μm, and hot strength is 15.43N, and elongation at break is 5.1%.
Embodiment
4
1) adding Kynoar, 1-METHYLPYRROLIDONE and polyethylene glycol (PEG-6000) in a kettle., mass ratio is 20:77:3, and at 55 DEG C, stirring makes it dissolve, and stirs 24h, forms uniform preparation liquid；
2) preparation liquid step 1) obtained filters through 200 mesh steel meshes, then by preparation liquid at room temperature vacuumizing and defoaming；
3) by step 2) preparation liquid after deaeration is at the N of 0.3MPa2Being extruded by spinneret under pressure, introduced by three glass fibres of a diameter of 0.1 μm of rolling in the preparation liquid of spinneret simultaneously, glass fibre constantly rotates under the effect of drawing head, around distribution and extrudes together with preparation liquid in the preparation liquid of spinneret；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane.
The enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane that embodiment 4 obtains, is filled with glass fibre, and glass fibre is around distribution, forms the reinforcement of three cinctures in its membranous wall；The porosity recording this enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane is 75%, and under 0.2Mpa permeable membrane pressure reduction, pure water flux is 165.13L m-2·h-1, average pore size is in 0.034 μm, and hot strength is 20.16N, and elongation at break is 5.0%.
Comparative example
1) adding Kynoar, 1-METHYLPYRROLIDONE and polyethylene glycol (PEG-6000) in a kettle., mass ratio is 20:77:3, and at 55 DEG C, stirring makes it dissolve, and stirs 24h, forms uniform preparation liquid；
2) preparation liquid step 1) obtained filters through 200 mesh steel meshes, then by preparation liquid at room temperature vacuumizing and defoaming；
3) by step 2) preparation liquid after deaeration is at the N of 0.3MPa2Extruded by spinneret under pressure；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain polyvinylidene fluoride hollow fiber ultrafiltration membrane.
The polyvinylidene fluoride hollow fiber ultrafiltration membrane that comparative example obtains is prior art products, does not fill enhancement fibrous material in its membranous wall；The porosity recording this polyvinylidene fluoride hollow fiber ultrafiltration membrane is 84%, and under 0.2Mpa permeable membrane pressure reduction, pure water flux is 195.42L m-2·h-1, average pore size is in 0.035 μm, and hot strength is 2.84N, and elongation at break is 7.2%.
Contrast from the product parameters of embodiment and comparative example and can be seen that, by filling enhancement fiber in the membranous wall of polyvinylidene fluoride hollow fiber ultrafiltration membrane, the hot strength making polyvinylidene fluoride hollow fiber ultrafiltration membrane is strengthened, and the parameter that the microcellular structure such as its porosity, pure water flux, average pore size is relevant simultaneously does not significantly change.It addition, the enhancement fiber around distribution more can be obviously enhanced film strength in the membranous wall of polyvinylidene fluoride hollow fiber ultrafiltration membrane.
In the present invention, enhancement fiber is not limited to the glass fibre enumerated in embodiment, the inorfils such as other carbon fibers, boron fibre, ceramic fibre, metallic fiber, the organic fibers such as aromatic polyamide fibre, superhigh molecular weight polyethylene fibers, Poly-p-phenylene benzobisthiazole, all can realize the purpose of the present invention.The diameter of enhancement fiber is preferably 0.1 ~ 10 μm.
In the present invention, preparation solvent used by enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane, additive, filming technology condition can use known conventional reagent and process conditions.
Finally illustrate is, preferred embodiment above is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail by above preferred embodiment, but skilled artisan would appreciate that, in the form and details it can be made various change, without departing from claims of the present invention limited range.
Claims (7)
1. an enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane, it is characterised in that: being filled with enhancement fiber in the membranous wall of described polyvinylidene fluoride hollow fiber ultrafiltration membrane, described enhancement fiber is cincture distribution in the membranous wall of polyvinylidene fluoride hollow fiber ultrafiltration membrane；The preparation method of described enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane comprises the following steps:
1) Kynoar, solvent and additive mix and blend are configured to preparation liquid；
2) deaeration after preparation liquid filtration step 1) obtained；
3) by step 2) preparation liquid after deaeration extruded by spinneret, and continuous print enhancement fiber is introduced in the preparation liquid of spinneret and extrudes together with preparation liquid simultaneously；
4) as-spun fibre that step 3) is extruded is immersed in coagulating bath and is frozen into hollow-fibre membrane；
5) put into the hollow-fibre membrane that step 4) obtains glycerin solution soaks and protect hole, be then placed in water soaking, obtain enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane；
In described step 3), enhancement fiber constantly rotates when introducing in the preparation liquid of spinneret, makes enhancement fiber around distribution in the preparation liquid of spinneret.
2. according to the enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane described in claim 1, it is characterised in that: described enhancement fiber is organic fiber or inorfil.
3. according to the enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane described in claim 2, it is characterised in that: described organic fiber is aromatic polyamide fibre, superhigh molecular weight polyethylene fibers or Poly-p-phenylene benzobisthiazole.
4. according to the enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane described in claim 2, it is characterised in that: described inorfil is glass fibre, carbon fiber, boron fibre, ceramic fibre or metallic fiber.
5. according to the enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane described in Claims 1-4 any one, it is characterised in that: a diameter of 0.1 ~ 10 μm of described enhancement fiber.
Enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane the most according to claim 1, it is characterized in that: in described step 1), the mass ratio of Kynoar, solvent and additive is 10 ~ 30:70 ~ 90:1 ~ 10, and the stirring preparation temperature of preparation liquid is 50 ~ 85 DEG C.
Enhancement polyvinylidene fluoride hollow fiber ultrafiltration membrane the most according to claim 1, it is characterized in that: in described step 1), solvent one in dimethylformamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, triethyl phosphate, trimethyl phosphate, hexamethyl ammonium phosphate, tetramethylurea, oxolane and acetone, additive one in polyvinylpyrrolidone, polyethylene glycol, lithium chloride, lithium perchlorate, glycerine, ethylene glycol, methyl alcohol, ethanol, water, formic acid and ethyl acetate.
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| CN106139920A (en) * | 2015-04-15 | 2016-11-23 | 辽宁纳诺膜科技股份有限公司 | A kind of high intensity, high water flux PVDF hollow-fibre membrane and preparation method thereof |
| CN106139919A (en) * | 2015-04-15 | 2016-11-23 | 辽宁纳诺膜科技股份有限公司 | A kind of hollow-fibre membrane with superelevation antifouling property and preparation method thereof |
| CN106731895A (en) * | 2015-11-19 | 2017-05-31 | 浙江省化工研究院有限公司 | A kind of preparation method of polyvinylidene fluoride hollow fiber microporous membrane |
| CN106040024B (en) * | 2016-06-24 | 2019-03-01 | 盐城海普润膜科技有限公司 | A method of producing inner support enhancement type hollow fiber film |
| CN106492645A (en) * | 2016-11-28 | 2017-03-15 | 天津工业大学 | Enhancement ultra-high molecular weight polyethylene and Kynoar binary blend film and preparation method thereof |
| CN110465201A (en) * | 2018-05-09 | 2019-11-19 | 湖州欧美新材料有限公司 | Aramid fiber ultrafiltration membrane and preparation method thereof |
| CN109173754B (en) * | 2018-08-23 | 2020-11-24 | 张妤涵 | Fluorine silicon film for high-salinity wastewater treatment and preparation method thereof |
| CN110813105A (en) * | 2019-11-12 | 2020-02-21 | 北京赛诺膜技术有限公司 | Preparation method and product of enhanced polyvinylidene fluoride hollow fiber membrane filament |
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| CN112044279A (en) * | 2020-09-17 | 2020-12-08 | 苏州关怀新材料技术研究有限公司 | Film making liquid for processing vaccine separation membrane and preparation method thereof |
| CN112844071A (en) * | 2020-12-24 | 2021-05-28 | 上海氧隆科技有限公司 | Preparation method of hollow fiber oxygen-enriched membrane |
| CN116492854B (en) * | 2023-06-07 | 2023-11-10 | 江苏诺莱智慧水务装备有限公司 | Hollow fiber ultrafiltration membrane production line and production method |
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| CN102266726A (en) * | 2011-08-23 | 2011-12-07 | 浙江大学 | Method for preparing long fiber reinforced hollow fibrous membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102266726A (en) * | 2011-08-23 | 2011-12-07 | 浙江大学 | Method for preparing long fiber reinforced hollow fibrous membrane |
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